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HRID246914

反应详情

EQUATION

反应方程式

HRID 246914 的结构方程式

REACTANTS

反应物

5
结构：CN(C)C=O
HCID6228

N,N-Dimethylformamide

C3H7NO

结构：CCN1CCOCC1
HCID7525

N-Ethylmorpholine

C6H13NO

结构：CCOC(C)=O
HCID8857

Ethyl acetate

C4H8O2

结构：CC(C)(C)OC(=O)N[C@@H](CCC(N)=O)C(=O)Oc1ccc([N+](=O)[O-])cc1
HCID7017891

L-Glutamine, N2-[(1,1-dimethylethoxy)carbonyl]-, 4-nitrophenyl ester

C16H21N3O7

结构：Oc1cccc2[nH]nnc12
HCID178418300

未命名化合物

PRODUCTS

生成物

1
结构：COC(=O)CNC(=O)[C@H](CCC(N)=O)NC(=O)[C@H](CCC(N)=O)NC(=O)OC(C)(C)C
HCID131714598

未命名化合物

收率 82%

PROCEDURE

实验过程

A solution of the residue obtained in the preceding step (theoretically 175.9 mM) in 500 ml of DMF, cooled on an ice bath, has 77.6 g of Boc-Gln-ONp (211.1 mM), 26.4 g of hydroxy benzotriazole (211.1 mM) and N-ethylmorpholine added thereto until a pH of 7 is obtained. After 20 hrs. of reaction at ambient temperature, the solution sets en masse. By addition of ethyl acetate, a precipitate is obtained which is drained, washed with AcOEt and dried in vacuo. 64.27 g of product are obtained, viz. a yield of 82%. Monitored by NMR and TLC.

WORKUP

后处理

  1. temperaturecooled on an ice bath
  2. additionadded
  3. customuntil a pH of 7 is obtained
  4. customof reaction at ambient temperature
  5. customa precipitate is obtained which
  6. washwashed with AcOEt
  7. customdried in vacuo